Impacts of Copper Surface Modification on the Cyclability and Estimation of Inactive Lithium in Anode-Free Lithium Metal Battery

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研究生：	Zewdu Tadesse Wondimkun Zewdu Tadesse Wondimkun
論文名稱：	Impacts of Copper Surface Modification on the Cyclability and Estimation of Inactive Lithium in Anode-Free Lithium Metal Battery Impacts of Copper Surface Modification on the Cyclability and Estimation of Inactive Lithium in Anode-Free Lithium Metal Battery
指導教授：	黃炳照 Bing-Joe Hwang
口試委員:	蘇威年 Wei-Nien Su 吳溪煌 Wu She-huang 周澤川 Chou Tse-Chuan .鄧熙聖 Hsisheng Teng 程敬義 Jim Cherng
學位類別：	博士 Doctor
系所名稱：	工程學院 - 化學工程系 Department of Chemical Engineering
論文出版年：	2020
畢業學年度：	108
語文別：	英文
論文頁數：	159
中文關鍵詞：	無陽極電池、人工固態電解質介面層、枝晶、氧化石墨烯、旋轉塗布、親鋰性、鋰金屬成核、奈米銀顆粒、聚多巴胺、電容量損失、失活鋰、酸鹼滴定、碘量滴定
外文關鍵詞：	Anode free battery, Artificial SEI, Dendrite, Graphene oxide, Spin coated, Lithiophilic, Lithium nucleation, Silver nanoparticles, Polydopamine, Capacity loss, Inactive lithium, Acid-base, Iodometric titrations
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鋰金屬電池被視為極具潛力的高能量密度儲能系統，然而，難以控制的鋰枝晶生長、死裡堆積、以及低庫倫效率限制其實際應用。諸多研究提出了不同方法用以抑制枝晶生長，例如微米/奈米結構鋰金屬負極、電解液添加劑形成穩定固態電解質介面層(SEI)、優化電解液溶劑、人工保護層、高濃度液態電解質、甚至是固態電解質。現今，無陽極鋰金屬電池(AFLMB)受到極大的關注，利用單純傳統氧化物正極材料與銅箔電流收集器作為電極，透過第一圈電池充電時臨場形成鋰金屬負極，不僅大幅增加能量密度、減少組裝成本、降低組裝繁瑣度，亦提升其安全性。然而，銅箔本身不親鋰、表面粗糙等特性，易造成鋰金屬沈積時產生電流分佈不均導致枝晶生長、死鋰累積、以及極高過電位導致電容量衰退等問題。而實質應用上，電容量衰退來自於死鋰的累積，如何有效且精準的量化死鋰亦是無陽極鋰金屬電池研究中有待解決得難題。
在本研究報導的第一個工作中，利用無需黏著劑之氧化石墨烯(Graphene oxide, GO)改質銅箔電流收集器，結合此平整且具導電度之人工固態電解質介面層與氟代碳酸乙烯酯(FEC)，鋰金屬沈積可以有效地被控制，進而得到平整、均勻、無枝晶的鋰沈積層。利用上述協同效應之無陽極鋰金屬電池可得到98%的平均庫倫效率，並且在50圈充放電後仍維持44%之初始電容量。對比無改質之對照組，平均庫倫效率只有89%並且在20圈後剩下26.9%之初始電容量。結果顯示GO塗布層與FEC添加劑可以有效的抑制鋰枝晶生長並且提升AFLMB的電化學效能。
在第二個工作中，具親鋰性的奈米銀-聚多巴胺顆粒(Ag@PDA)成功被製備並塗布於銅箔表面作為核點以促進鋰金屬沉積成核，接著塗布前一工作之GO於表面作為復合人工SEI促進鋰離子分佈，達到均勻沈積與抑制枝晶生長之協同效應。利用Cu|Ag@PDA//Li與Cu|Ag@PDA-GO//Li電池組成進行測試，從結果得知此改質後之桐柏具有更均勻核點、低成核過電位、以及較高的庫倫效率。此外，Cu|Ag@PDA-GO//NMC無陽極鋰金屬電池產出更高之庫倫效率(~98.6%)，並且在60圈循環後維持55.7%之初始電容量。因此，利用復合型親鋰人工SEI塗布層可以有效的抑制枝晶生長以及電解液分解。
於最後一個工作中，一個簡單、低成本、嚴謹的酸鹼與碘量滴定被第一次報導應用於量測死鋰於使用不同電解液之AFLMB中產生的數量。結果顯示於不同電解液配方中，導致電容量衰退與堤庫倫效率的原因來自於被SEI包覆不具電化學活性的鋰金屬(死鋰)，且死鋰的數量與電解液配方非常相關。此滴定技術與結果對於死鋰定量分析開啟一個新的方向。

Lithium metal battery (LMB) is a promising high-energy-density energy storage system. However, the unregulated growth of lithium dendrite, dead lithium accumulation, and low Coulombic efficiency (CE) upon cycling is hampering the applications of LMBs. Numerous strategies, for instance, constructing micro/nanostructured lithium metal anodes, using stable SEI layer forming additives, optimizing electrolyte solvent, introducing artificial SEI film, coating separators with high infiltrated material, high concentrated electrolytes, and solid-state electrolytes have been suggested to mitigate lithium dendrite. Currently, anode free battery (AFB), which is constructed from bare copper and lithium containing cathode material, can be used as an alternative strategies to minimize the direct use of Li anode. AFB configuration is a promising approach to enhance energy density, reduce cost, and enable ease cell fabrication with safety. Nevertheless, the Li metal plating onto the bare Cu surface became inhomogeneous and results in the formation of lithium dendrite and dead lithium accumulation due to the heterogeneous, rough, and lithiophobic properties of the bare Cu. Moreover, the battery possesses a substantial nucleation barrier that leads to much higher overpotential and quick capacity loss. The capacity loss results from the inactive (dead) lithium accumulation luck exact quantification tools.
In the first part, the copper current collector was modified with a binder-free ultra-thin spin-coated graphene oxide (GO). The synchronized smooth and conductive GO-coated artificial SEI with lithium fluoride derived from fluoroethylene carbonate (FEC) electrolyte additive greatly control the lithium deposition. Accordingly, the synergistic effect of GO and LiF-rich inherent SEI enables smooth, uniform, and dendrite-free lithium plating. Moreover, the AFB with GO film and 5% FEC in the carbonate-based electrolyte is capable of achieving high Coulombic efficiency of an average 98% and attains ~44% of its initial capacity after 50 cycles. In contrast, the full cell with bare Cu//LiNi1/3Mn1/3Co1/3O2 (NMC) has a Coulombic efficiency of 89% and retains 26.9% after 20 cycles. These results show that GO-coated artificial SEI with FEC additive can be a promising approach to impede lithium dendrites growth and result in enhanced electrochemical performance in an AFB.
In the second work, lithiophilic silver nanoparticles with polydopamine (Ag@PDA) were synthesized and coated on the copper substrate to use as a nucleation seed, which improves the lithium nucleation in anode free lithium metal batteries (AFLMBs). Interestingly, graphene oxide (GO) was coated on the top of Ag@PDA to act as an artificial SEI and buffer the Li-ion distribution. Thus, the modified electrodes show a uniform Li metal deposition and dendrite free morphology upon repeated cycling. Accordingly, the Cu|Ag@PDA//Li, and Cu|Ag@PDA-GO//Li cells demonstrate relatively uniform lithium nuclei, lower nucleation overpotential, and higher CE compared to the uncoated electrode. Besides, the Cu|Ag@PDA-GO//NMC full cell has higher average Coulombic efficiency (~ 98.6%) and higher capacity retention (~ 55.7%) after 60 cycles within 1 M LiPF6 EC/DEC (1:1 vol. %) + 5% FEC at 0.5 mA cm-2. In contrast, the cell with bare copper only offers 94.4% and 4.3% average CE and capacity retention, respectively. Therefore, a lithiophilic matrix integrated with an artificial SEI coating on the Cu substrate offers a feasible way for the inhibition of lithium dendrite and electrolyte decomposition in the anode free lithium metal batteries (AFLMBs).
In the final work, acid-base and iodometric titrations techniques are established for the first time to estimate the amounts of inactive (dead) lithium on Cu current collector using 1 M LiPF6 1:1 (EC: DEC), 1 M LiPF6 1:1 (EC: DEC) + 5% FEC, and 1 M LiPF6 5:3:2 (TTE: FEC: EMC) electrolytes in AFLMBs. Consequently, very comparative results are attained in both techniques in Cu// NMC cell using those electrolytes at the 1st and 20th cycle. The findings confirmed that the capacity loss and lower CE were mainly caused by the electrically inaccessible unreacted metallic Li (Li0) compared to the formation of solid electrolyte interphase (SEI) in all electrolyte systems. Besides, the amounts of dead lithium accumulated on the Cu surfaces are highly dependent on the types of electrolytes used. When using electrolyte consisting of FEC and partially fluorinated ether-based solvent (TTE), which can form a LiF rich SEI, the accumulation of inactive lithium became lowered compared to the commercial electrolytes. Moreover, the inactive lithium accumulated is consistent with the cyclic performances of the cells. The result opens up a new direction to realize the estimation of inactive (dead) lithium by using simple, versatile, low-cost, and consistent titrations techniques.

Contents
中文摘要    iii
Abstract    v
Acknowledgments    viii
List of Figures    xv
List of Schemes    xx
List of Tables    xxi
Chapter 1: Introduction    1
1    Background of the study    1
2 Rechargeable batteries as energy storage device    2
3 Lithium-ion rechargeable battery system    4
Chapter 2: The fundamentals of lithium metal and anode free lithium metal batteries    8
1 The lithium metal batteries    8
2 Challenges faced by Li metal anodes    8
2.1 The harsh reactivity of Li metal    9
2.2 Volume expansions in Li metal during cycling    10
2.3 The formation of lithium dendrites and dead lithium    10
2.4 The SEI and failure of the Li metal anode    11
3 Approaches to inhibit Li dendrite formation in lithium metal batteries    12
3.1 Electrolyte formulation    12
3.2 Solid-state electrolyte (SSEs)    13
3.3 Electrolyte additive    14
3.4 Separator/membrane modification    15
3.5 Ex situ-formed surface coating    16
3.6 Effect of pressure    16
4 Anode free lithium metal batteries configuration    18
4 Current progress of lithium metal anode free batteries    20
5 Estimation of inactive lithium in anode free lithium metal batteries    27
6 Motivation and objectives of the study    31
6.1 Motivations    31
6.2 Objectives    32
Chapter 3: Experimental Sections    33
1 Chemicals and Reagents    33
2 The synthesis of polydopamine coated silver nanoparticles (Ag@PDA)    34
3 Electrodes preparation    34
3.1 Electrodes preparation    35
3.2 Preparation of GO coated copper electrode    35
3.3 Fabrication of Ag@PDA and Ag@PDA-GO coated Cu electrodes    36
4 Preparation of electrolytes    36
5 Preparation of standard, analyte, indicators and samples for dead lithium estimations    37
5.1 Preparation of 0.01 M HCl titrant    37
5.2 Preparation of sodium thiosulphate (0.01 M Na2S2O3) titrant    37
5.3 Preparation of triiodide solution    37
5.4 Preparation of starch indicator    38
6 Electrochemical measurement and characterization    38
6.1 Electrochemical tests    38
6.2 Characterizations    39
6.3 Dead lithium estimation    40
Chapter 4: Binder-free ultra-thin graphene oxide as an artificial solid electrolyte interphase for anode-free rechargeable lithium metal batteries    42
1 Introduction    42
2 Results and Discussion    45
2.1 Modified electrode morphology and thickness evolution    45
2.2 Effects of coating on the cyclic performances    47
2.3 Electrochemical impedance spectroscopy and cyclic voltammetry analysis    54
2.4 The effect of coating on the lithium morphology    57
2.5 Analysis of surface chemistry    62
3 Summary    68
Chapter 5: Highly-lithiophilic Ag@PDA-GO film to suppress dendrite formation on Cu substrate in anode-free lithium metal batteries    69
1 Introduction    69
2 Results and Discussion    72
2.1 Characterization of AgNPs and Ag@PDA    72
2.2 Morphology evaluation of the modified electrodes    74
2.3 Effects of Ag@PDA and Ag@PDA-GO coating on the cyclic performance of the cells    77
2.4 Assessments of lithiophilicity    84
2.5 Assessments of wettability    86
2.6 Small-Angle X-Ray Scattering (SAXS) analysis    87
2.7 Effects of Ag@PDA-GO of coating on the morphology of Li deposition    90
2.8 Electrochemical impedance spectroscopy measurements    94
2.8 Mechanical and chemical stability test of the modified electrodes    95
3 Summary    99
Chapter 6: Estimation of dead lithium on Cu Current Collector at different electrolyte system in AFLMBs    100
1 Introduction    100
2 Results and Discussion    102
2.1 Cyclic performance for inactive lithium evaluations    102
2.2 Morphology and inactive Li evaluation with different electrolytes    104
2.3 Acid-base titration for estimation of dead lithium    106
2.4 Iodometric titration for the estimation of dead lithium    111
2.5 MAS NMR analysis of inactive lithium (Li0 and Li+) in Cu//NMC cells    118
3 Summary    120
Chapter 7: Conclusions and Future Perspectives    121
1 Conclusions    121
2 Future perspectives    124
References    125
Appendixes    135


                                

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